New high surface area carbon materials were prepared at low temperature (600 °C) using zeolite (Y, Beta, and ZSM-5) and montmorillonite clay (K10) templates. Acrylonitrile, furfuryl alcohol, pyrene, and vinyl acetate precursors were polymerized and carbonized in each of the inorganic matrixes without the addition of a polymerizing agent. The templates were removed by acid demineralization and the resulting carbon materials were physically characterized by infrared spectroscopy, BET (N 2 ) surface area analysis, energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM), and elemental analyses. Electrochemical characterizations were also conducted. Cyclic voltammetry was employed to examine the synthesized carbons in the oxidation of catechol to hydroquinone and quinone, a model reaction that is known to be surface dependent. The identities of both the template and the substrate affected the electrochemical response. Additionally, the ability of the new carbons to intercalate and deintercalate lithium was investigated. While all of the synthesized carbons displayed high irreversible capacities consistent with other low-temperature carbons, the carbons prepared from zeolite Y displayed unique voltage curves, suggesting template effects on the carbon. In addition, all of the carbons prepared for this study displayed significant voltage hysteresis on charge/discharge.
EuS nanoparticles were synthesized by solution-phase thermolysis of the diethylammonium salt of the anionic europium dithiocarbamate complex, [Eu(S 2 CNEt 2 ) 4 ] -. Oleylamine and triphenylphosphine were used as surfactants to prevent nanoparticle agglomeration and stabilize particle growth. By varying the synthetic parameters such as reaction temperature, heating time, and the [surfactant]:[precursor] ratio, nanoparticles of different sizes were obtained. The size-dependent magnetic properties of these nanoparticles were studied, and it was observed that a decrease in the ferromagnetic ordering temperature occurs with decreasing particle size.
A simple and straightforward method of depositing nanostructured thin films, based on LiCl-doped TiO 2 , on glass and LiNbO 3 sensor substrates is demonstrated. A spin-coating technique is employed to transfer a polymer-assisted precursor solution onto substrate surfaces, followed by annealing at 520°C to remove organic components and drive nanostructure formation. The sensor material obtained consists of coin-shaped nanoparticles several hundred nanometers in diameter and less than 50 nm thick. The average thickness of the film was estimated by atomic force microscopy (AFM) to be 140 nm. Humidity sensing properties of the nanostructured material and sensor response times were studied using conductometric and surface acoustic wave (SAW) sensor techniques, revealing reversible signals with good reproducibility and fast response times of about 0.75 s. The applicability of this nanostructured film for construction of rapid humidity sensors was demonstrated. Compared with known complex and expensive methods of synthesizing sophisticated nanostructures for sensor applications, such as physical vapor deposition (PVD) and chemical vapor deposition (CVD), this work presents a relatively simple and inexpensive technique to produce SAW humidity sensor devices with competitive performance characteristics.
Metal-oxo clusters have been used as building blocks to form hybrid nanomaterials and evaluated as potential MRI contrast agents. We have synthesized a biocompatible copolymer based on a water stable, nontoxic, mixed-metal-oxo cluster, Mn8Fe4O12(L)16(H2O)4, where L is acetate or vinyl benzoic acid, and styrene. The cluster alone was screened by NMR for relaxivity and was found to be a promising T2 contrast agent, with r1 = 2.3 mM(-1) s(-1) and r2 = 29.5 mM(-1) s(-1). Initial cell studies on two human prostate cancer cell lines, DU-145 and LNCap, reveal that the cluster has low cytotoxicity and may be potentially used in vivo. The metal-oxo cluster Mn8Fe4(VBA)16 (VBA = vinyl benzoic acid) can be copolymerized with styrene under miniemulsion conditions. Miniemulsion allows for the formation of nanometer-sized paramagnetic beads (~80 nm diameter), which were also evaluated as a contrast agent for MRI. These highly monodispersed, hybrid nanoparticles have enhanced properties, with the option for surface functionalization, making them a promising tool for biomedicine. Interestingly, both relaxivity measurements and MRI studies show that embedding the Mn8Fe4 core within a polymer matrix decreases r2 effects with little effect on r1, resulting in a positive T1 contrast enhancement.
We have prepared gadolinium doped europium sulfides, Eu(1-x)Gd(x)S for a doping range of 0 ≤ x ≤ 0.1 by thermal decomposition of the precursors Eu(S(2)CNEt(2))(3)Phen/Gd(S(2)CNEt(2))(3)Phen with respective ratios. Electron doping provides indirect evidence for the magnetic coupling through carrier electrons in magnetic semiconductors. Based on the magnetic properties, we determined that the paramagnetic Curie temperature, Θp, varies with doping level, in a similar way to Eu(1-x)Gd(x)O exhibiting a significant increase at low doping levels. All materials have been characterized by X-ray powder diffraction, magnetic measurements, ICP-MS, and TEM.
Lead iodide nanoparticles are synthesized in reverse micelle solution of AOT/H2O/n-heptane. Optical absorption spectra and TEM analysis indicated the formation of crystalline particles with an average radius of 1.5 nm, which is less than the Bohr radius of the exciton (1.9 nm) in bulk PbI2. Using theoretical models and optical spectra of quantum confined PbI2 nanoparticles, a radius of 1.5 nm and a thickness of 1.7 nm was calculated, which are in full agreement with the TEM results. Particles were isolated from the dispersed medium and were analysed by powder XRD and Raman spectroscopy, indicating the formation of a predominantly 2H-PbI2 polytype. This work presents the first case of fully isolated, fully characterized solid nanoparticles of PbI2. It also presents XRD and Raman spectrum for the first time for PbI2 nanoparticles of intermediate quantum confinement.
We have previously reported the cloning of the Salmonella enterica serovar Typhimurium SPI-1 secretion system and the use of this clone to functionally complement a ΔSPI-1 strain for type III secretion activity. In the current study, we discovered that S. Typhimurium cultures containing cloned SPI-1 display an adherent biofilm and cell clumps in the media. This phenotype was associated with hyper-expression of SPI-1 type III secretion functions. The biofilm and cell clumps were associated with copious amounts of secreted SPI-1 protein substrates SipA, SipB, SipC, SopB, SopE, and SptP. We used a C-terminally FLAG-tagged SipA protein to further demonstrate SPI-1 substrate association with the cell aggregates using fluorescence microscopy and immunogold electron microscopy. Different S. Typhimurium backgrounds and both flagellated and nonflagellated strains displayed the biofilm phenotype. Mutations in genes essential for known bacterial biofilm pathways (bcsA, csgBA, bapA) did not affect the biofilms formed here indicating that this phenomenon is independent of established biofilm mechanisms. The SPI-1-mediated biofilm was able to massively recruit heterologous non-biofilm forming bacteria into the adherent cell community. The results indicate a bacterial aggregation phenotype mediated by elevated SPI-1 type III secretion activity with applications for engineered biofilm formation, protein purification strategies, and antigen display.
Comparative studies are presented of iron oxide nanoparticles in the 7-15 nm average diameter range ball milled in hexane in the presence of oleic acid. Transmission electron microscopy identified spherical particles of decreasing size as milling time and/or surfactant concentration increased. Micromagnetic characterization via Mössbauer spectroscopy at room temperature yielded broadened magnetic spectroscopic signatures, while macromagnetic characterization via vibrating sample magnetometry of 7-8 nm diameter particles showed largely superparamagnetic behavior at room temperature and hysteretic at 2 K. Zero-field and field-cooled magnetization curves exhibited a broad maximum at ∼215 K indicating the presence of strong interparticle magnetic interactions. The specific absorption rates of ferrofluids based on these nanoparticle preparations were measured in order to test their efficacies as hyperthermia agents.
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